Apparatus for determining ash.



No. 665,04|. Patented Ian. I, ram.

(5. mgrucxea. v APPARATUS FOR DETERMINING ASH.

(Application filed pee. 1a. 1899.) (No Model.) 2 Sheats-8heet I.

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No. 665,04l. Patented Jan. I, 190:.

G. M. TUCKER.

APPARATUS FOR DETERMINING ASH. (Application filed Dee. 1a, 1899.)

(No Model.) 2 $heats-8haeh 2.

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UNITED STATES PATENT OFFIcE.

GEORGE MASON TUCKER, OF KINGSTON, RHODE ISLAND.

APPARATUS FOR DETERMINING 'ASH.

SPECIFICATION forming part of Letters Patent No. 6 da d n ry 1, 1901- Application filed December 18, 1899. Serial No. 740,657. kNo model.)

To all whom it may concern.-

Beitknown thatLG oReEMAsoN TUCKER, a citizen of the United States, and a resident of Kingston, Rhode Island, have invented a new and useful Improvement in Apparatus for Determining the Total Ash of Any 0 rganic Matter, of which the following is a specification.

The object of the invention is to provide a novel and convenient apparatus for making quantitative determinations of ash obtained from various materials, as well as of other materials than ash. The apparatus may also be used for the dry distillation of substances and may also be employed for the production of iodin where this material is obtained by burning sea-weed, inasmuch as by such apparatus as is at present employed the seaweed is burned in the open and much iodin escapes as gas.

In the accompanying drawings, Figure 1 represents the apparatus as arranged for preliminary charring of the substance. Fig. 2 represents the apparatus as finally arranged for the purpose of determining the crude ash. Fig. 3 is an enlarged section on the line w a: of the tube M and cup supported thereon. Fig. 4 is an enlarged sectional view of the beaker and aspirator. V

Similar characters of reference indicate like parts.

Referring first to Fig. l, A is a cylinder, of sheet-iron, supported upon legs B and provided with a n umber of smallppenings around its periphery, as shown at 0. Supported within the cylinder A by means of its flanges, which rest upon the upper edge of said cylinder, is a sheet-iron dish D in the form of an inverted conical frustum.

E is a cover which fits over the flange of the dish D and is made, preferably, of nickel. In the center of this cover is secured a smokestack F, preferably of brass. Through the cover are made four holes, which receive short flanged tubes, of brass, two of which are shown at G. These tubes fit so tightly in the openings of the cover that while they can be moved up and down they will be held firmly in any position in which they may be placed.

Any suitable heating device, such as a Bunsen gas-burner H, is to be placed below the cylinder A, so that its flame will surround the dish D and the heated air will escape at the openings 0. The part of my apparatus so far described I will call the oven.

I is a crucible-shaped platinum dish, preferably two and one-half cubic meters in diameter at the bottom. This dish is shown somewhat enlarged in Fig. 2. The sides are drawn in slightly at J.

K is a platinum cover for the dish I, which must be made to fit said dish as nearly airtight as possible. Secured in said cover are two platinum tubes L and M. The tube L when the cover is in place extends down nearly to the bottom of the dish and receives the vertical rod N of the stirrer. The stirrer consists of the vertical rod N, which is provided with an upper square portion 0 to receive a key for turning said rod and with bent arms P, which arms extend radially at the lower part of the dish and then upward in line parallel to the side. On the under side of the cover and surrounding the protruding end of the tube Mis a thin platinum ring Q. The extremity of the tube M is provided with a rim R, in which rim are diametrically opposite recesses S, Fig. 3.

T is a small platinum cup having on the inner periphery of its upper edge two projections U. The mouth of the cup is inserted between the tube and the ring Q, so that the projections U enter the recesses S. Then by turning the cup around the projections U come above the rim R of the tube, and in this Way the cup is detachably supported in place.

V is a platinum beaker, through the rub ber stopper W of which passes the bent-over end of the tube M or, preferably, an added tube Z, which extends below the level of the surface of the liquid in beaker V. Communicating with the space above the liquid within beaker V is a tube Y, the outer end of which may communicate with any suitable form of aspirator. Such a form of aspirator is illustrated in Fig. 4, which consists of an ordinary glass bottle 2, through the stopper 3 of which are inserted two tubes, one of which, 4, extends nearly to the bottom of the bottle. The tube 4 connects with the tube Y, as shown. The other tube 5 is provided with a stop-cock 6. The bottle contains water or other suitable liquid. In order to draw air through the apparatus, the stop-cock 6 is opened and the water in the bottle 2 allowed to run out in the ordinary way.

The apparatus is to be used in the following manner: The complete apparatus, (shown in Fig. 2,) excepting stopper W and tubes Y and Z, being previously weighed, the finelypowdered material to be burned is put into dish I. The dish Iis then placed upon enough sand in the dish D of Fig. 1 to raise the dish I nearly to the cover of the dish D. Then sand is poured around the edges between the two dishes as high as the angle in the dish I. It will be observed that the slope of the Wall of the lower portion of the dish I is greater than that of the wall of the dish D, so that the thickness of the space between the two dishes gradually diminishes, and also that the total depth of the dish I is less than that of the dish D. This admits of a thick layer of sand at the bottom between the dishes, where the heat is the highest, and the gradual decrease of said layer between the two dishes as the heat decreases due to the greater distance of the parts of the apparatus from the flame. In this way a nearly-uniform temperature is produced within the dish I. The small bottom and sloping sides of the dish D admit of its being completely enveloped by the flame, thus obtaining sufficient heat at the point farthest from the burner to char fully the particles within the dish I which are most remote. This construction of my apparatus oifers an import-ant advantage over apparatus in which the dish has a flat bottom and vertical sides, inasmuch as in such case it is impossible to produce sufficient heat at the surface of the material within the inner dish without having a great heat at the bottom, which may drive the easily-volatile substances into the air. The object of the tubes G is to admit a free circulation of air in contact with the material to be reduced to ash, and thus to facilitate rapid combustion. When the material has been brought to a dark-colored ash, which usually requires less than an hour, the platinum dish I is removed and set into a proper-sized hole in an asbestos sheet a, Fig. 2. This sheet is to be supported in any suitable manner in such a way as to cause it to protect the upper part of the apparatus from the heat of the flame. The flame maybe derived from a Bunsen burner H, as shown, arranged below the platinum dish I. The stirrer N is then introduced into the dish I and the cup T is disposed in place to cover the end of the tube M. The function of this cup is to prevent the particles of ash escaping through the tube M. The cover K is then placed firmly upon the dish and the end of tube M connected, preferably, to a bent tube Z. entering beaker V. The aspirator is then operated to produce an inward current of air through tube L for the rapid oxidation of the material in crucible I. Heat is now gradually applied at the bottom of dish I until the whole wall of the dish in contact with the material is brought to a red heat. The material is stirred from time to time by means of the stirrer. The nature of the material treated determines the length of time of application of the heat, as well as the intensity of the heat to be applied. As soon as the ash becomes whitethat is, as soon as the material has become reduced to a good ash-the source of heat is removed, the air-current cut off, the connections of beaker V broken, the tubes Y an d Z are washed with a few drops of water into beaker V, which is then set in a water-bath and evaporated to dryness,and the parts weighed, as before. As the ash is-weighed in a closed dish, fluctuations due to taking in moisture from the air are avoided. Deducting the weight of the empty apparatus from the combined weight of apparatus and contents gives the weight of the crude ash. Carbonic-acid gas may be determined without removing the ash from the dish I. For this purpose the cover is removed and the parts are washed carefully with distilled water into the dish. The cup T and stirrer N are removed and put one side. The cover K is then replaced and the edge is sealed, preferably by means of a rubber band stretched around the overlapping edge of the cover. The tube M is then connected with the usual apparatus for collecting carbonic-acid gas, and dilute hydrochloric acid is introduced into the dish I through the tube L. Afterthe completion of this operation the contents of the crucible may be subjected to the usual analysis.

The principal advantages of this apparatus are the following: There is absolutely no loss of volatile substances, such as chlorids of potassium, sodium, phosphoric acid, oxids of sulfur, dac. These are either sublimed on the walls of the apparatus or else caught in the liquid in the beaker V. The substances can be reduced to ash very rapidly, as the necessary heat is quickly applied without danger of loss of the volatile substances. The tedious process of washing out the volatile substance before the completion of the burning process is avoided. Carbonic-acid gas may be determined without removing the ash from the apparatus, and thus a possibility of error is avoided. As the ash is made and weighed in a closed dish, the weight is not appreciably affected by atmospheric moisture. The form of the dish admits of a more uniform and therefore a more rapid charring, while the tubes in the cover of the oven allow a more complete circulation of air, thus hastening combustion. The gaseous products of combustion are drawn through a liquid. Therefore in the apparatus as arranged in Fig. 2 the pressing tendency is toward its interior, and consequently there can be no escape of combustion-gases around the edge of the cover. As the stirring-rod passes through the air-tube, the latter cannot be choked at the bottom by the substance so as to exclude the air. The sloping sides of the dish permit of a more perfectly fitting cover and also one that can readily be removed as desired. The general construction and arrangement are such-that none of the volatile substances escape.

I claim- 1. The combination of the crucible I having an inwardly-inclined upper portion J, the cover K adapted to fit on said portion J, the tube L and gas-escape pipe M secured in said cover and the stirrer-rod N received in said tube L and provided with arms P, substantially as described.

2. The combination with an aspirator for withdrawing volatile products of the crucible I, cover K, tube M, secured in said cover, and communicating with said aspirator, and

communicating with said aspirator and a detachable cup T within said crucible and arranged to cover the tube-opening, substantially as described.

GEORGE MASON TUCKER.

Witnesses:

M. F. PERRY, H. J. WHEELER. 

